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Hydrochloric Acid → HCID 21956378, 화합물

HRID 989291
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반응식

HRID 989291 반응식
C([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][C:11]([Cl:20])=[C:12]([N+:17]([O-:19])=[O:18])[CH:13]=2)[NH:8][CH:7]=1)=[O:5])C.[OH-].[Na+].Cl>C(O)C>[Cl:20][C:11]1[CH:10]=[C:9]2[C:14]([C:15](=[O:16])[C:6]([C:4]([OH:5])=[O:3])=[CH:7][NH:8]2)=[CH:13][C:12]=1[N+:17]([O-:19])=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 127338527-Chloro-6-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester

생성물 1

HCID 21956378HCID 21956378, 화합물수율 92.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 12.0 g (40.5 mmol) of 7-chloro-6-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid ethyl ester (J. Med. Chem. 23, 1358 (1980)) and 60.0 mL of 2.5 N sodium hydroxide in 160.0 mL of ethanol is heated at reflux temperature for 1.5 hours. After allowing the reaction mixture to cool to room temperature, it is further cooled in an ice bath, brought to pH 4 with 4.0 N hydrochloric acid and stirred for 0.5 hour. The solid is collected by filtration, washed with water and dried in vacuo to yield 10.1 g of 7-chloro-6-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid as a tan solid, mp 294-297° C.

후처리

  1. temperatureis heated
  2. temperatureat reflux temperature for 1.5 hours
  3. temperatureit is further cooled in an ice bath
  4. filtrationThe solid is collected by filtration
  5. washwashed with water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-ef4b4aa6f4154d1c95bd7ead7e94518e
출처 데이터셋
uspto-grants-2003_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06638929B2

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